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Preparation method of monoclinic phase yttrium oxide

A technology of yttrium oxide and monoclinic phase, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of incapable mass production and high pressure, and achieve the effect of simple and efficient synthesis method, low preparation conditions and high product purity

Pending Publication Date: 2018-11-09
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the high pressure required by this method, only a small amount of research can be carried out, and it cannot be used in large batches for production.

Method used

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  • Preparation method of monoclinic phase yttrium oxide
  • Preparation method of monoclinic phase yttrium oxide
  • Preparation method of monoclinic phase yttrium oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0022] (1) Preparation of yttrium-based coordination polymer: 0.5mmol Y(NO 3 ) 3 ·6H 2 O and 1.5mmol oxalic acid were dissolved in 40ml of DMF solvent, and reacted in a household microwave reaction device for 15min with a power of 240W;

[0023] (2) Cubic phase Y 2 o 3 Preparation: The yttrium-based coordination polymer obtained by microwave reaction was calcined in a muffle furnace for 4 hours, and the calcination temperature was 800°C;

[0024] (3) Cubic phase Y 2 o 3 The precompression of: the cubic phase Y obtained after calcination 2 o 3 Put it into Mo package and pre-press, and the loading pressure is 10MPa;

[0025] (4) High temperature and high pressure reaction: the pre-pressed cubic phase Y 2 o 3 , the reaction was carried out in a domestic hinged 1400-ton six-sided top press. First, the pressure was raised to 3GPa at a rate of 0.3GPa / min. After the pressure was stabilized, the temperature was raised to 1000°C at a rate of 100°C / min and kept for 0.5h. , th...

Embodiment 2

[0028] (1) Preparation of yttrium-based coordination polymer: 0.1mmol Y(NO 3 ) 3 ·6H 2 O and 0.3 mmol terephthalic acid were dissolved in 40 ml DMF and H 2 In a mixed solvent of O, react in a household microwave reaction device for 20min with a power of 240W;

[0029] (2) Cubic phase Y 2 o 3 Preparation: The yttrium-based coordination polymer obtained by microwave reaction was calcined in a muffle furnace for 4 hours, and the calcination temperature was 1000°C;

[0030] (3) Cubic phase Y 2 o 3 The precompression of: the cubic phase Y obtained after calcination 2 o 3 Put in Pt package and pre-press, the loading pressure is 5MPa;

[0031] (4) High temperature and high pressure reaction: the pre-pressed cubic phase Y 2 o 3 , the reaction was carried out in a domestic hinged 1400-ton six-sided top press. First, the pressure was raised to 5GPa at a rate of 0.5GPa / min. After the pressure was stabilized, the temperature was raised to 1000°C at a rate of 50°C / min and kept f...

Embodiment 3

[0034] (1) Preparation of yttrium-based coordination polymer: 0.475mmol Y(NO 3 ) 3 ·6H 2 O, 0.025mmolEu(NO 3 ) 3·6H 2 O and 0.3mmol pimelic acid were dissolved in 40ml of DMF solvent, and reacted in a household microwave reaction device for 15min with a power of 240W;

[0035] (2) Cubic phase Y 2 o 3 : Eu 3+ Preparation: The europium-doped yttrium-based coordination polymer obtained by microwave reaction was calcined in a muffle furnace for 4 hours, and the calcination temperature was 800°C;

[0036] (3) Cubic phase Y 2 o 3 : Eu 3+ The precompression of: the cubic phase Y obtained after calcination 2 o 3 : Eu 3+ Put it into Mo package and pre-press, and the loading pressure is 10MPa;

[0037] (4) High temperature and high pressure reaction: the pre-pressed cubic phase Y 2 o 3 : Eu 3+ , the reaction was carried out in a domestic hinged 1400-ton six-sided top press, and the pressure was first raised to 3GPa at a rate of 0.3GPa / min. After the pressure was stabili...

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Abstract

The invention provides a preparation method of monoclinic phase yttrium oxide. The preparation method comprises the following steps: (1) preparing a yttrium-base coordination polymer; (2) calcining the yttrium-base coordination polymer, so as to obtain cubic phase yttrium oxide; (3) pre-pressing cubic phase yttrium oxide at 2MPa-20MPa; and (4) carrying out high-temperature and high-pressure reaction on pre-pressed cubic phase yttrium oxide at 500-1500 DEGC and 1GPa-5GPa, so as to obtain monoclinic phase yttrium oxide. The preparation method has a series of advantages of simple process, relatively low reaction condition, high product purity and yield and the like. According to the preparation method, a rapid and efficient novel method is provided for the synthesis of monoclinic phase yttrium oxide.

Description

technical field [0001] The invention relates to the technical field of preparation of rare earth oxides, in particular to a method for preparing monoclinic yttrium oxide. Background technique [0002] In the research of various rare earth materials, the preparation and application of rare earth oxides have always been the key research objects, because of their wide application in optics, catalysis, magnetism, etc., researchers have generally paid attention to them. Among them, half-fold rare earth oxides exhibit different crystal structures under different external conditions, including cubic, monoclinic, hexagonal, etc. In terms of the crystal structures of these compounds, at ambient temperature and pressure, they are known to exist in three structural modifications, namely A, B and C, corresponding to the hexagonal structure (space group P3m1 in most cases), single Oblique phase (space group C2 / m in most cases) and cubic phase (space group Ia3 in most cases). As the fir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/505C04B35/622C09K11/78
CPCC04B35/505C04B35/622C04B2235/6562C04B2235/6565C04B2235/6567C04B2235/76C09K11/7787
Inventor 钟声亮李欣炜夏先明刘冉
Owner JIANGXI NORMAL UNIV
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